HRID26499

反应详情

EQUATION

反应方程式

HRID 26499 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

To 2.3 g of 8-chloro-3-methylsulfonyl-11H-s-triazolo[3,4-b][3]benzazepine in 20 ml of dioxane was added 10 ml of 2N-potassium hydroxide and the mixture was heated on a water bath at 95° C. for 30 minutes. The solvent was evaporated off and water was added to the residue. The mixture was made acidic with 2N-HCl and the resultant crystalline precipitate was recovered by filtration and dried. By the above procedure was obtained 8-chloro-2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one as crystals. Recrystallization from chloroform-methanol yielded colorless platelets, m.p. 281°-283° C.

WORKUP

后处理

  1. customThe solvent was evaporated off
  2. additionwater was added to the residue
  3. filtrationthe resultant crystalline precipitate was recovered by filtration
  4. customdried